This invention pertains to the preparation of di-tertiary peroxides and more particularly to the removal of water by chemical reaction in situ.
Di-tertiary alkyl or aryl peroxides have been prepared by the condensation of a hydroperoxide and an alcohol in the presence of an acid catalyst. This reaction is depicted in equation (1) below: EQU ROOH+R'OH.sup.H.spsp.+ ROOR'+H.sub.2 O (1)
It has been demonstrated in such syntheses as the preparation of dicumyl peroxide from cumene hydroperoxide and cumyl alcohol that the removal of the water formed in reaction (1) facilitates the reaction especially by reducing the reaction time needed to reach a given conversion of reactants to products. This permits, for example, increased production capacity from a given reactor. However, all of the prior art methods for removing this water of reaction have called for the use of either physical separation or the formation of physically hydrated species with an anhydrous substance. Thus, for example, sulfuric acid has been used as a dehydrating agent by Y. Tsunoda, Nippon Kagaku Zasshi, 81, 310 (1960), nitrogen gas has been bubbled through the reaction mixture by Y. Tsunoda, Kogyo Kagaku Zasshi, 63, 837 (1960), reduced pressure has been used to remove water as disclosed in U.S. Pat. Nos. 3,337,639 and 3,308,163, and azeotropic agents have been used to remove water as disclosed in Canadian Pat. No. 839,312, U.S. Pat. Nos. 3,584,057, 3,337,369, 3,308,163 and 3,681,316. Dihydrates have been formed using anhydrous oxalic acid, as disclosed in U.S. Pat. No. 3,310,558. Dried silica-alumina was used in Japanese Pat. No. 15,970 (1964) (Chemical Abstracts 62:10376e). Anhydrous magnesium sulfate was used to remove water as a hydrate as disclosed in U.S. Pat. No. 3,833,664.